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WO2006080535A1 - Phosphore rouge de nitrure et procédé de fabrication de celui-ci - Google Patents

Phosphore rouge de nitrure et procédé de fabrication de celui-ci Download PDF

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Publication number
WO2006080535A1
WO2006080535A1 PCT/JP2006/301595 JP2006301595W WO2006080535A1 WO 2006080535 A1 WO2006080535 A1 WO 2006080535A1 JP 2006301595 W JP2006301595 W JP 2006301595W WO 2006080535 A1 WO2006080535 A1 WO 2006080535A1
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Prior art keywords
red phosphor
phosphor
powder
activated
raw material
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PCT/JP2006/301595
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Japanese (ja)
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WO2006080535A9 (fr
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Shin-Ichi Sakata
Takeshi Yamao
Tetsuo Yamada
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Ube Industries, Ltd.
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Priority to JP2007500656A priority Critical patent/JP5045432B2/ja
Priority to US11/795,298 priority patent/US8148886B2/en
Priority to EP06712738.1A priority patent/EP1845146B1/fr
Priority to CN2006800016380A priority patent/CN101090953B/zh
Publication of WO2006080535A1 publication Critical patent/WO2006080535A1/fr
Publication of WO2006080535A9 publication Critical patent/WO2006080535A9/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/0883—Arsenides; Nitrides; Phosphides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0602—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with two or more other elements chosen from metals, silicon or boron
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Definitions

  • the present invention relates to a nitride red phosphor used for a display, a backlight for liquid crystal, a fluorescent lamp, a white light emitting diode, and the like, and a method for producing the same.
  • White light-emitting diodes are lightweight, do not use mercury, and have a long lifetime, so demand is expected to grow rapidly in the future.
  • YA activated with cerium G Y 3 A 1 5 0 2:! C e
  • the paste of the mixture of powder and epoxy resin was applied to the blue color light emitting element is employed (Japanese Patent Laid-Open No. 2 0 00-2 0 8 8 1 "5).
  • An object of the present invention is to provide a new nitride red phosphor that absorbs blue light and emits red fluorescence. Disclosure of the invention
  • the present inventors proceeded with a detailed study of phosphors activated by Eu in the calcium nitride (C a 3 N 2 ) -aluminum nitride (A 1 N) —silicon nitride (Si 3 N 4 ) system. It was. As a result, we found the presence of red phosphors excited by blue light, which is different from the previously reported C a A 1 Si N 3. Thus, according to the present invention, the following is provided.
  • a 1 N is not detected by X-ray diffraction analysis Red color as described in (3) Phosphor.
  • the average particle diameter measured by the laser diffraction / scattering particle size distribution measurement method is 10 or less, and is activated by Eu, and is a C a A 1 Si N a powder.
  • a characteristic red phosphor is 10 or less, and is activated by Eu, and is a C a A 1 Si N a powder.
  • red phosphor which is a C a A l S i N 3 powder pulverized that has been activated by E u described.
  • a light emitting device including a light emitting element, a yellow phosphor, and the red phosphor according to any one of (1) to (7).
  • FIG. 1 is a triangular diagram showing the composition range of the raw material powder of the present invention and the compositions of Examples and Comparative Examples.
  • FIG. 2 is an X-ray diffraction pattern of the powder of the fired product obtained in Example 1.
  • FIG. 3 is an X-ray diffraction pattern of the powder obtained by acid cleaning of the fired product of Example 1.
  • FIG. 4 is a comparison of X-ray diffraction patterns of the powders of Example 1 and Comparative Example 9.
  • FIG. 5 is a comparison of X-ray diffraction patterns of the powders of Example 1 and Comparative Example 9.
  • FIG. 6 is a fluorescence spectrum diagram of the nitride red phosphor of the present invention obtained in Example 1.
  • FIG. 7 is an excitation spectrum diagram of the nitride red phosphor of the present invention obtained in Example 1.
  • FIG. 8 is an X-ray diffraction pattern of the powder of the fired product obtained in Example 2.
  • FIG. 9 is a comparison of X-ray diffraction patterns of the powders of Example 2, Example 1 and Comparative Example 9.
  • FIG. 10 is a comparison of X-ray diffraction patterns of the powders of Example 2, Example 1, and Comparative Example 9.
  • FIG. 11 is an X-ray diffraction pattern of the powder of the fired product obtained in Example 3.
  • FIG. 12 is an X-ray diffraction pattern of the fired powder obtained in Comparative Example 1.
  • FIG. 13 is an X-ray diffraction pattern of the fired powder obtained in Comparative Example 2.
  • FIG. 14 is an X-ray diffraction pattern of the fired powder obtained in Comparative Example 3.
  • FIG. I 5 is an X-ray diffraction pattern of the powder of the fired product obtained in Comparative Example 4.
  • FIG. 16 is an X-ray diffraction pattern of the powder of the fired product obtained in Comparative Example 5.
  • FIG. 17 is an X-ray diffraction pattern of the powder of the fired product obtained in Comparative Example 6.
  • FIGS. 21A and 21B are scanning electron micrographs showing the morphology of the particles in Example 4 and Comparative Example 10 respectively.
  • FIG. 23 shows the fluorescence spectrum of the particles of Example 4.
  • Figure 24 shows the excitation spectrum of the particles of Example 4.
  • FIG. 25 shows a lamp using a light emitting diode and a red phosphor as an example of the light emitting device of the present invention.
  • nitride red phosphor of the present invention and the method for producing the same are described below.
  • FIG. 3 shows an X-ray diffraction pattern of the red phosphor according to the first aspect of the present invention (hereinafter also simply referred to as “the red phosphor of the present invention”).
  • the method disclosed in the 6th 5th JSAP Academic Lecture Meeting, Proceedings of Lectures 1 2 8 3 (hereinafter referred to as “Literature 1”) C a A 1 Si N 3
  • the X-ray diffraction pattern was measured (Comparative Example 9). The results are shown in FIG.
  • the X-ray diffraction pattern of Fig. 20 was compared with the diffraction pattern of C a Al Si N 3 disclosed in Ref.
  • FIG. 3, Example 1 the red phosphor of the present invention
  • C a Al Si N 3 FIG. 20, Comparative Example 9
  • the X-ray diffraction patterns in Fig. 3 and Fig. 20 are very similar but differ greatly in detail. This will be described.
  • Figure 4- compares the 2 ⁇ (hereinafter the same) between 30 ° and 42 °.
  • the red phosphor of the present invention has a peak around 31.5 °, 36.3 . Nearby peaks are split and peaks different from C a A 1 S i N 3 appear.
  • Figure 5 shows a comparison from 45 ° to 70 °. Here too, there is a split at the peak near 5 6.2 °.
  • the diffraction patterns from 68 ° to 69 ° differ greatly. From the above, the red phosphor of the present invention is different from the C a A l S i N 3 red phosphor disclosed in the literature 1.
  • Table 2 shows the composition analysis results of the red phosphor of the present invention.
  • Table 2 also shows the theoretical percentage of each element of C a Al Si N 3 for comparison.
  • the analysis value of the red phosphor of the present invention is very close to C a Al Si N 3 . Considering that complete quantitative analysis is very difficult, it can be considered that the composition of this phosphor is almost C a A 1 Si N 3.
  • this red phosphor is C a Al Si N 3 belonging to the monoclinic system.
  • Eu is substituted for a part of C a site. The amount of substitution is within the range of 0.1 to 8.8 mol% with respect to the Ca site 0.1 to 5.0 mol% and further 0.8 to 3.0 mol%. preferable.
  • FIG. 6 The fluorescence spectrum when excited by the blue light of 4500 nm of the invention is shown.
  • the wavelength of fluorescence generated by excitation with blue is 660 nm (red) and is suitable as a red phosphor with blue light excitation. For this reason, it can be used as a red phosphor used for color tone control for a white light emitting diode in which a blue light emitting diode and YAG: Ce are combined.
  • Figure 7 shows the excitation spectrum when the fluorescence wavelength is set to 660 nm. This phosphor shows high emission from 3 0 0 11 111 to 5 2 0 11 111, indicating that it can be used as a good phosphor in the ultraviolet to blue region.
  • the internal quantum efficiency of the phosphor of the present invention was measured.
  • the phosphor of Reference 1 Comparative Example 9
  • the quantum efficiency of the phosphor of Comparative Example 9 is set to 100
  • the quantum efficiency of the phosphor of the present invention is 1 1 7
  • C a A 1 Si N 3 belonging to the monoclinic system of the present invention is This was confirmed to be a better phosphor (see Table 3).
  • the method for producing the red phosphor of the present invention will be described.
  • the nitride materials involved in the manufacture of nitride phosphors are described.
  • raw materials Ca 3 N 2 , Eu N, A 1 N, and Si 3 N 4 are used.
  • any method can be adopted as long as the nitride can be finally obtained.
  • a typical method for producing raw materials is described.
  • C a 3 N 2 can be produced by directly nitriding metallic calcium.
  • Calcium metal is placed in a carbon or BN crucible and heated at 60 ° C. to 90 ° C. and then nitrided.
  • calcium nitride is commercially available, and a commercially available product (for example, manufactured by Aldrich) may be used.
  • E u N can also be obtained by direct nitridation of metallic europium.
  • Metal europium is atomized with a jar in a nitrogen box, Place in a carbon or BN crucible. This is put in a firing furnace and heated at 600 to 900 ° C. in a nitrogen atmosphere to perform nitriding.
  • a part of E u N may be substituted with E u 2 O 3.
  • a 1 N a force that employs a direct nitriding method or a reductive nitriding method of alumina, a high-purity A I N force, which is widely available on the market, may be used.
  • Akuma N 1 F F grade
  • F grade a force that employs a direct nitriding method or a reductive nitriding method of alumina
  • Si 3 N 4 powder can be obtained by a known method.
  • nitrogen-containing silanes such as silicon nitride produced by reacting halogenated silicon such as tetrachlorosilane, tetratetrabromide and tetraiodide with ammonia in the gas phase or liquid phase.
  • Amorphous silicon nitride can be obtained by a method of thermally decomposing at 0 ° C. or a method of reacting gaseous halogen halide with ammonia at a high temperature. Furthermore, crystalline silicon nitride can be obtained by baking this amorphous silicon nitride at 140 ° C. to 160 ° C. in a nitrogen atmosphere.
  • nitride red phosphors of the present examples are C a 3 N 2 , E u N, A 1 N, S
  • 1 3 N 4 is used as a raw material, and the desired weight is weighed, mixed, and then fired in a nitrogen atmosphere.
  • composition range of the raw material for producing the nitride red phosphor of the present invention is indicated by hatching in the composition diagram of FIG.
  • the shaded area is the following four points A to D, that is, a straight line connecting four points where the molar ratio of (C a 3 N 2 : A 1 N: Si 3 N 4 ) is the following ratio. It is an area surrounded by.
  • Point B (1 0: 6 5: 2 5)
  • Point C (7 0: 2 3: 7)
  • composition is XC a 3 N 2 yA 1 N z z S i 3 N 4 (+ y + z
  • the red phosphor according to the present invention has the best strength when the molar ratio between the forces A 1 N and Si 3 N 4 of 3: 1 can be obtained by using the raw materials having the above composition range. If it is in the range of 1, it is preferable.
  • the force that C a 3 N 2 is in the range of 10 to 70 mol% of the total of 100 mol% of the raw material powders Ca 3 N 2 , A 1 N, and Si 3 N 4 S, 2
  • a range of 0 to 40 mol% is preferable.
  • the method of mixing each starting material described above there is no particular limitation on the method of mixing each starting material described above, and a method known per se, for example, a dry mixing method, a wet mixing in an inert solvent that does not substantially react with each component of the raw material, and then the solvent is added.
  • the removal method can be adopted.
  • a V-type mixer, a rocking mixer, a pole mill, a vibration mill, a medium stirring mill, etc. are preferably used.
  • the mixture of starting materials can be baked in a nitrogen-containing atmosphere at 14 00 to 20 00 to obtain the target phosphor.
  • the target phosphor can be obtained by baking at 150 ° C. to 1700 ° C. If the firing temperature is lower than 140 ° C., it takes a long time to produce the desired phosphor, which is not practical. In addition, the production rate of the phosphor in the produced powder decreases. If the firing temperature exceeds 1800 ° C., calcium and europium may evaporate remarkably and a bright phosphor may not be obtained.
  • the nitrogen-containing atmosphere may contain, in addition to nitrogen, an inert gas in the sense that it does not affect the composition of the nitride red phosphor of the present invention, for example, a rare gas, an argon gas, a helium gas, etc.
  • an inert gas in the sense that it does not affect the composition of the nitride red phosphor of the present invention
  • nitrogen-containing atmosphere a nitrogen atmosphere and a mixed atmosphere of nitrogen and an inert gas can also be referred to as “nitrogen-containing inert atmosphere.
  • the starting raw material mixed powder can also be fired in a temperature range of 16 00 to 20 00 ° C., preferably 16 00 to 19 00 ° C., under a pressurized nitrogen gas atmosphere.
  • pressurization of nitrogen gas suppresses evaporation of calcium and europium and sublimation decomposition of Si 3 N 4 , and a desired phosphor can be obtained in a short time.
  • the firing temperature can be increased by increasing the nitrogen gas pressure. For example, it is 160 to 180 ° C. under a nitrogen gas pressure of 5 atm, and 16 0 0 under a nitrogen gas pressure of 10 atm. Baking can be performed at 0 to 200 ° C.
  • the heating furnace used to fire the powder mixture for example, a batch-type electric furnace, rotary kiln, fluidized firing furnace, pusher-type electric furnace using a high-frequency induction heating method or a resistance heating method. Etc. can be used.
  • the method for producing a nitride red phosphor according to the present invention has the composition range shown in FIG. A mixture of C a 3 N 2 , A 1 N, and Si 3 N 4 represented by the following formula: A raw material obtained by adding 0.001 to 10 parts by weight to 100 parts by weight of EuN as Eu The powder is calcined at 140 ° C. to 200 ° C. in a nitrogen-containing atmosphere. Further, it is preferable that the nitrided red phosphor after firing is further acid washed to remove the remaining unnecessary oxide. Next, the nitride red phosphor of the present invention will be described.
  • the nitride red phosphor of the present invention has a composition consisting of C a 3 N 2 , A 1 N, and Si 3 N 4 represented by the composition range (shaded area) in FIG.
  • C a A 1 Si N 3 which is the main component and activated by monoclinic Eu.
  • This nitride red phosphor absorbs at least a portion of the first emission spectrum having a peak wavelength in the range of 2700 to 5200 nm, and has a wavelength of 580 to 6800 nm.
  • a second emission spectrum having a peak wavelength in the range can emit light.
  • Nitride red phosphor of the present invention can be obtained similarly by using the raw material partially substituted with E u 2 03 in E u N. Therefore, the red phosphor of the present invention may have a small amount of oxygen.
  • Calcium oxide may remain in the above-mentioned calcined product.
  • CaO it can be removed by washing with an acid, so there is no problem. If the composition range is out of the above range, sufficient emission intensity cannot be obtained even if the target phosphor cannot be obtained or the target phosphor can be obtained.
  • a composition containing a large amount of A 1 N also causes a problem that A 1 N remains in the phosphor after firing. A 1 N cannot be removed by washing with acid like Ca 0, and is not preferable when used as a phosphor.
  • the nitride red phosphor of the present invention is activated by monoclinic Eu. a A 1 Si N 3 force that does not contain free AIN can be obtained. In particular, X-ray diffraction analysis can be obtained that does not contain an A 1 N peak. However, the content of A 1 N in the nitride red phosphor is
  • the present invention provides a light emitting device (such as a lamp) in which the above-described nitride red phosphor is combined with a light emitting element, in particular, a blue light emitting element and a red phosphor. Since the nitride red phosphor of the present invention is excited by blue and can emit red fluorescence with high efficiency, a blue light emitting device and a red phosphor
  • the monoclinic C a A 1 was partially replaced with E u is S i N 3, and C a A 1 S i N 3 monoclinic are all novel crystalline It is considered to be a substance. It is clear that monoclinic C a Al Si N 3 can be produced in the same way without partial substitution with Eu.
  • an average particle diameter measured by a laser diffraction / scattering particle size distribution measurement method is 10 or less, and activated by Eu.
  • red phosphor is S i N 3 powder
  • to provide a red phosphor is a C a a 1 S ⁇ ' ⁇ 3 powder pulverized that has been activated by the E u of ⁇ benefactor.
  • C a A 1 S i ⁇ 3 activated by Eu can also be a monoclinic crystal.
  • Ca Al S i N 3 is composed of 2 to 3 primary particles assembled to form secondary particles.
  • Reference 2 It has been pointed out that phosphors for white light-emitting diodes may cause uneven light emission and products due to non-uniform phosphor arrangement when extremely large particles are included. (Material Integration V ol. 1 6, No. 7 (2 0 0 3), page 4 1). For this reason, the presence of large secondary particles contained in C a Al Si N 3 is not preferable. In order to eliminate the large secondary particles, a method of pulverizing after the powder production can be considered. However, generally, when the phosphor powder is dusted, there arises a problem that the emission intensity decreases.
  • the present inventors consider that the aggregate particles in C a Al Si N 3 are caused by the generation of a glass phase by a slight amount of oxygen contained in the raw material and the adhesion of the crystal particles through the formation of the glass phase.
  • C a Al Si N 3 was prepared using few crystalline nitrides.
  • no improvement effect is seen, and only powder containing large secondary particles can be produced.
  • aggregated particles are formed by another mechanism in addition to the above-mentioned aggregation of primary particles being bonded via a composition that forms a glass like oxygen. is doing.
  • the primary particle agglomeration forms primary secondary particles that are in close contact with each other (see Fig.
  • the primary particles come into contact with the surface when C a A 1 Si N 3 nucleates.
  • each crystal nucleus is thought to be caused by a dense spatial nucleation. This can be attributed to the fact that the entire raw material is dense, that is, the bulk density of the raw material is high. It is also important to prevent the formation of C a A 1 Si N 3 crystal nuclei from occurring in a specific location.
  • As a method for solving such a problem if amorphous silicon nitride or a nitrogen-containing silane compound that is a precursor thereof is used as a raw material for nitride nitride, there is little aggregation of primary particles and large secondary particles are obtained.
  • the inventors have found that a Ca A 1 Si N 3 phosphor powder can be obtained that has been greatly reduced, and have reached the second aspect of the present invention.
  • the C a A 1 Si N 3 powder according to the second aspect of the present invention can be produced by using amorphous nitride nitride (amorphous nitride) as a raw material for C a Al Si N 3 .
  • Amorphous silicon nitride has a very low bulk density of about 0.1 lg / cc.
  • crystalline silicon nitride is about 0.7 g / cc, which is about 7 times the volume of the same weight.
  • the bulk density of the raw material powder is much higher than that when crystalline silicon nitride is used. It becomes small and becomes a bulky powder. For this reason, when C a Al Si N 3 forms crystal nuclei, it can spatially separate and nucleate. In addition to spatial factors, the size of crystalline nitride formed from amorphous nitride is considered to have an effect.
  • this raw material powder containing amorphous silicon nitride is heated in a nitrogen atmosphere, the crystallization temperature of the nitride nitride is lower than the reaction temperature of Ca A 1 Si N 3 , Nucleates to crystalline silicon nitride. In this case, the step size is very small compared to crystalline silicon nitride. On the floor, it becomes possible to contact other raw material components such as C a 3 N 2 and A 1 N. For this reason, uniform nucleation of C a A 1 Si N 3 occurs when amorphous silicon nitride is used.
  • the method for producing the C a A 1 Si N 3 powder of the second aspect of the present invention may be the same as the production method described in the first aspect except for the above.
  • EuN is added to 100 parts by weight of a mixture consisting of C a 3 N 2 20 mol%, A 1 N 60 mol%, and Sia N 4 20 mol%. It can be produced by firing raw material powder mixed with 0.01 to 10 parts by weight as Eu in a nitrogen-containing inert atmosphere at 140 to 180 ° C.
  • Amorphous nitride (amorphous nitride) is replaced with C a A l S i N
  • the average particle diameter measured by the laser diffraction / scattering degree distribution measurement method is 10 m or less in the state of green powder.
  • C a A 1 S i activated by Eu red phosphor is N 3 powder, and can provide a red phosphor is a powder ⁇ of C a a l S i N 3 ' powder activated with E u of that.
  • the second light-emitting spectrum having a peak wavelength in the range of 5880 to 680 nm can emit light.
  • This red phosphor is a fine and uniform C a A 1 Si N 3 powder without using powder powder. Even when grinding, the degree of grinding The 90% diameter can be reduced to 45 xm or less, preferably 20 m or less. Therefore, the decrease in emission intensity due to powder can be eliminated or reduced.
  • Figure 25 shows an example of a lamp using the nitride red phosphor of the present invention.
  • the light emitting diode 2 on the substrate 1 is connected to the lead 4 through the gold wire 3.
  • the light emitting diode 2 is embedded in a resin 6 containing a nitride red phosphor of the present invention and YAG activated by Ce in a container 5.
  • the nitride red phosphor absorbs part of the light and emits red light.
  • Y AG Ce absorbs part of the blue light and emits yellow light.
  • Fig. 1 shows the composition points of each example and comparative example. Table 1 also shows that the raw material composition ratios of Examples and Comparative Examples are not 7 pieces. table 1
  • Si 3 N 4 powder was prepared as follows. Silicon diimide obtained by reacting silicon tetrachloride with ammonia at a temperature below room temperature was heat-treated at 120 ° C. to obtain amorphous nitride nitride powder, which was used as a raw material. Regarding the A 1 N powder, a commercially available product (F grade) manufactured by Tokama Corp. was used.
  • Figure 2 shows the X-ray diffraction pattern of this powder. From the X-ray pattern, although A 1 N was not present, C aO remained (Ca 0 was identified using In 0 rganic Crystal Structure Data collection code 7 5 7 8 5). In Fig. 2, the position of the peak that can be separated as CaO is indicated by an arrow. As mentioned above, C aO remains This powder was washed with a 2N nitric acid solution to remove CaO. Fig. 3 shows the X-ray diffraction pattern of the phosphor powder thus obtained.
  • FIG. 3 a detailed comparison of the red phosphor of the present invention (FIG. 3) Der red phosphor of Comparative Example 9 and Ruhasukata crystal C a A l S i N 3 ( Fig. 2 0).
  • the X-ray diffraction patterns in Fig. 3 and Fig. 20 are very similar but differ greatly in detail.
  • Fig. 4 expands the X-ray diffraction pattern of 2 S force from 30 ° to 42 °
  • Fig. 5 expands the diffraction pattern of 2 ⁇ from 45 ° to 70 °.
  • the peak near 31.5 ° and the peak near 36.3 ° are split, and a peak different from orthorhombic Ca A 1 Si N 3 appears.
  • Figure 4 shows a comparison from 45 ° to 70 °. Here too, splitting is observed at the peak near 56.2 °. Furthermore, the diffraction patterns from 68 ° to 69 ° differ greatly. From the above, it is considered that the red phosphor of the present invention is different from the red phosphor disclosed in the red phosphor of Comparative Example 9 (the same as in Reference 1).
  • the quantum efficiency was obtained using the same device and the quantum efficiency measurement program.
  • the results were evaluated as relative values, assuming that the internal quantum efficiency of orthorhombic C a A 1 Si N 3 of Comparative Example 9 was 1 0 0.
  • the results are shown in Table 3.
  • the quantum efficiency is superior to that of the orthorhombic system, and it was found that the red phosphor of the present invention has excellent characteristics.
  • Got. Figure 8 shows the X-ray diffraction pattern of this powder.
  • FIG. 9 shows an enlarged view of the portion of 2 S from 30 ° to 42 °.
  • the X-ray diffraction pattern of this powder is shown in Fig. 11. Although C a O remains, the X-ray diffraction pattern excluding C a 0 is the same as in Example 1. This red phosphor is monoclinic C a A 1 Si N 3 It was confirmed.
  • this red phosphor contains CaO, it was washed with an acid in the same manner as in Example 1 to remove CaO, and a fluorescence spectrum and an excitation spectrum were measured in the same manner as in Example 1. The result was the same fluorescence spectrum and excitation spectrum as in Example 1. Furthermore, the internal quantum efficiency was determined by the same method as in Example 1. The red phosphor was also excellent red phosphor than C a A l S i N 3 orthorhombic.
  • phosphor powders were produced in the same manner as in Example 1.
  • Figure 12 shows the X-ray diffraction pattern. From the analysis of the X-ray diffraction pattern, it was confirmed that the red phosphor crystal of Example 1, CaO, and A1N were present in this powder. As in Example 1, it was possible to remove C aO by washing with 2N nitric acid, but A 1 N could not be removed. When the fluorescence spectrum was measured, the fluorescence wavelength was almost the same as in Example 1. The emission intensity is about 50% of that in Example 1.
  • phosphor powders were produced in the same manner as in Example 1.
  • Fig. 16 shows the X-ray diffraction pattern. From the analysis of this X-ray diffraction pattern, this powder has an orthorhombic C a A 1 Si N 3 in Comparative Example 9. (Lattice constants are different) There were crystal phases and crystal phases that could not be identified. A very small amount of A 1 N was also present.
  • the fluorescence spectrum was measured, the fluorescence wavelength was shifted to yellow as compared with Example 1 and was 6500 nm. The emission intensity was about 66% of Example 1.
  • phosphor powders were produced in the same manner as in Example 1.
  • Figure 17 shows the X-ray diffraction pattern. From the analysis of this X-ray diffraction pattern, the powder had an orthorhombic C a A 1 Si N 3 (differing lattice constant) crystal phase in Comparative Example 9 and an unidentifiable crystal phase.
  • the fluorescence wavelength was 645 nm, shifted to yellow compared to Example 1.
  • the emission intensity was about 50% of Example 1.
  • FIG. 21A A scanning electron micrograph (hereinafter referred to as SEM photograph) of the phosphor powder prepared in Example 2 is shown in FIG. 21A.
  • Fig. 21B shows a photograph of the morphology of the particles when crystallized nitride nitride is used.
  • Fig. 2 In C a A 1 Si N 3 using 1 B crystalline nitride nitride, the primary particles are in contact with the surface and become strongly agglomerated secondary particles of about 10 ⁇ m.
  • 2 1 A amorphous nitride nitride is used as the raw material, no large secondary particles in which the primary particles are in close contact with each other and in close contact are observed. If you look in detail, Fig.
  • FIG. 21A also shows agglomerated particles as shown in Fig. 21B, but its size is much smaller than Fig. 21B.
  • the individual particles of C a A 1 Si N 3 produced using amorphous nitride nitride are self-shaped. This suggests that C a A 1 S i N 3 was crystallized in a spatially isolated field ', which we have envisioned, with the crystal nuclei spatially separated and uniformly nuclei. It confirms that it was formed.
  • the fluorescence spectrum of the obtained phosphor was measured at an excitation wavelength of 45 Onm.
  • F P 6500 with integrating sphere manufactured by JASCO Corporation was used, and the measurement spectrum was corrected using a sub-standard light source.
  • the results are shown in Figure 23. 6 8 8 nm red light emission was confirmed, and this nitride red phosphor was confirmed to be suitable as a phosphor for adjusting the color tone of a white light emitting diode using a blue light emitting diode.
  • Comparative Example 9 was repeated. That is, a phosphor was fabricated by the same method as in Example 2 except that crystalline nitride nitride was used as the silicon nitride raw material. The specific surface area of the crystalline silicon nitride used was about 10 m 2 / g. The oxygen content was 1.3 wt%.
  • FIG. 21B An SEM photograph of the obtained powder C a A 1 Si N 3 particles is shown in FIG. 21B. In order to clearly show the basic structure of the particles, Then, a small particle was chosen and shown. Actually, the particles are mainly larger than those shown in the photograph. The large existence form was that particles as shown in Fig. 21 B were further connected to form large particles.
  • Example 4 the fluorescence spectrum and the excitation spectrum were measured by the same method as in Example 4. As a result, a peak position equivalent to that in Example 4 was obtained, but the fluorescence intensity was lower than that in Example 4.
  • the particle size distribution measurement was performed in the same manner as in Example 4.
  • C a A 1 Si N 3 produced using crystalline silicon nitride had many lumps of about several hundreds m that were relatively hard and sintered.
  • the lumps were crushed using an agate mortar.
  • the measurement results are shown in Fig. 22.
  • the average particle size was 29.3 xm.
  • the phosphor powder of Comparative Example 10 has many powders of 60 im or more. These huge particles are not suitable as phosphor powders for white light emitting diodes. In order to use this powder as a phosphor for a white light emitting diode, it is necessary to grind.
  • Comparative Example 1 1 A phosphor was fabricated in the same manner as in Comparative Example 10 except that crystalline nitride nitride containing less oxygen was used as the nitride nitride raw material.
  • the crystallized nitride used had a surface area of about 3 m 2 Zg and an oxygen content of 0.9 wt%.
  • the silicon nitride powder used in this comparative example was used, the bulk density of the raw material powder was larger than that of Comparative Example 10, and the powder was low in bulk.
  • the average particle diameter of the obtained powder is shown in Table 4.
  • Comparative Example 1 the particles were large aggregated particles.
  • the fluorescence spectrum and the excitation spectrum were lower than in Example 2.
  • this powder also needs to be pulverized in order to be used as a phosphor for a white light emitting diode.
  • a phosphor was produced in the same manner as in Example 2 except that the added EuN was changed to 2.5 parts by weight as Eu.
  • the fluorescence wavelength of the obtained phosphor was shifted to the long wavelength side compared with Example 2 and became 66.66 nm.
  • Table 3 shows the results of measuring the quantum efficiency of this phosphor by the same method as in Example 1.
  • a phosphor was prepared in the same manner as in Example 2 except that the added Eu Eu was changed to 11 parts by weight as Eu, and the fluorescence spectrum was measured in the same manner as in Example 2. The fluorescence wavelength was shifted to 69 4 nm. The fluorescence intensity decreased to 50% of Example 2. '' Industrial applicability
  • the present invention it is possible to provide a novel and efficient nitride red phosphor that absorbs blue light and emits red fluorescence.
  • the nitride red phosphor does not show unnecessary light emission because it contains almost no residual A 1 N phase.
  • the red phosphor of the present invention does not contain coarse particles even if it is not powdered, it can prevent a decrease in luminous efficiency when pulverized. It is a red phosphor with high luminous efficiency.
  • the nitride red phosphor can be combined with a light emitting element such as a light emitting diode to provide a light emitting device with excellent color tone.

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Abstract

L’invention concerne un phosphore rouge dont la phase cristalline constituant le phosphore se compose de CaAlSiN3 activé par Eu monoclinique. En particulier, elle porte sur un phosphore rouge caractérisé en ce qu’il se compose de poudre de CaAlSiN3 activé par Eu d’un diamètre particulaire moyen, sous forme non pulvérisée mesuré par le procédé de mesure de répartition de taille particulaire par diffraction/dispersion laser, ≤ 10 µm. Elle concerne en outre un élément luminescent comprenant un élément luminescent bleu, le phosphore rouge ci-dessus étant capable de convertir une lumière bleue émise par l’élément luminescent bleu en lumière rouge et un phosphore jaune capable de convertir la lumière bleue en lumière jaune. Elle concerne en outre un procédé de fabrication de CaAlSiN3 activé par Eu, consistant à cuire dans une atmosphère azotée à 1400 - 2000°C une poudre de matière première de Ca3N2, AlN et Si3N4 dont la composition entre dans la fourchette définie dans le schéma de composition de la Fig. 1 par des lignes droites reliant quatre points A à D chacun représenté par (Ca3N2 : AlN : Si3N4) où le rapport molaire moyen de Ca3N2, AlN et Si3N4 est le suivant : Point A: (10:70:20), Point B: (10:65:25), Point C: (70:23:7) et Point D: (70:22:8), la poudre de matière première contenant en outre de l’EuN dans une quantité comprise entre 0,01 et 20 parties en poids en termes d’Eu pour 100 parties en poids du total de Ca3N2, AlN et Si3N4.
PCT/JP2006/301595 2005-01-31 2006-01-25 Phosphore rouge de nitrure et procédé de fabrication de celui-ci WO2006080535A1 (fr)

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JP2007500656A JP5045432B2 (ja) 2005-01-31 2006-01-25 赤色蛍光体の製造方法および赤色蛍光体
US11/795,298 US8148886B2 (en) 2005-01-31 2006-01-25 Red nitride phosphor and production method thereof
EP06712738.1A EP1845146B1 (fr) 2005-01-31 2006-01-25 Luminophore de nitrure émettant dans le rouge et procede de fabrication de celui-ci
CN2006800016380A CN101090953B (zh) 2005-01-31 2006-01-25 红色氮化物荧光材料及其制造方法

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TW200632071A (en) 2006-09-16
MY149962A (en) 2013-11-15
CN101090953B (zh) 2012-10-03
EP1845146A1 (fr) 2007-10-17
US8148886B2 (en) 2012-04-03
EP1845146B1 (fr) 2015-03-04
US20080128726A1 (en) 2008-06-05
TWI374927B (en) 2012-10-21
JPWO2006080535A1 (ja) 2008-06-19
CN101090953A (zh) 2007-12-19
WO2006080535A9 (fr) 2010-09-16
JP5045432B2 (ja) 2012-10-10

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